Comminuted drying oil residues



Jan, 18, 1949. w. F. SCHAUFELBERGER 2,459,342

COMHINUTED DRYING OIL RESIDUES Filed March 8, 1944 ZNDENSER R5051 VER Ram/2 Aa/rA 7'02 VACUUM A INVENTOR. WILLIAM E SCHAUFELBERGER BY 5- Q Patented Jan. 18, 1949 COMMINUTED DRYING OIL RESIDUES William F. Schaufelberger, Pleasant Grove, N. J assignor to Irvington Varnish and Insulator Company, a corporation of New Jersey Application March 8, 1944, Serial No. 525,615

8 Claims.

The present invention relates to comminuted, infusible, non-oxidized residues obtained by heating certain drying oils in vacuo with accompanying agitation and to a method of obtaining such residues.

It has previously been known that a few drying oils, such as China-wood oil and oiticica oil, can be polymerized to solid gels upon heating, even in substantial absence of air. Such oils are characterized by the presence of conjugated double bonds, combined with a low content of saturated fatty acid glycerides. In the case of the other known drying oils, polymerization by heat alone produces liquid products of increased viscosity.

Thus the treatment of drying oils by heating in vacuo has been utilized by the paint and varnish industry for the preparation of light-colored bodied oils of improved drying characteristics. In such treatments, the temperatures have been held between 500 and 600 F. to avoid appreciable decomposition of the glyceride oils. It has been found in the course of the present investigation that by using drying oils which are polymerized to liquid products by heat alone, solid, comminuted products are obtained by raising the temperature of the oil to 610 F. and higher, preferably not above 700 F., together with the application of suction and with the aid of agitation. Appreciable decomposition occurs, a liquid condensate is collected and a comminuted, infusible residue ob tained. The oils found suitable for the practice of this invention are those glyceride oils having an iodine number in excess of 120 (Wijs), substantially free of conjugated double bonds and further characterized by conversion to liquid products of higher viscosity by heat alone. Examples of such oils are linseed oil, sardine oil, menhaden oil, pilchard oil, sunflower oil, Perilla oil, soya bean oil, walnut oil, hempseed oil, poppyseed oil and corn oil. Oils such as China-wood oil and oiticica oil which can be polymerized to solid gels by heat alone are not suitable for the purposes of this invention and the claims have been so drawn as to exclude them from the scope of the invention.

The products of the method of this invention are (1) a liquid or pasty condensate, alcohol soluble and of high acid value and consisting chiefly of fatty acids and (2) a comminuted, infusible, non-oxidized residue varying in texture from a soft, rubbery to a hard, horny particle. The residue constitutes l90% by weight of the original material.

The latter products, which are the subject of this invention, may be used, for example, as rubber substitutes with the addition of adequate fillers and vulcanizers, in brake linings, clutches and other friction element facings and as binders for the abrasive materialsof grinding wheels.

The superior advantages of these products in brake linings and the like spring from their infusibility combined with low volatility at operating temperatures.

In addition, there are advantages inherent in the process of producing these products which overcome difliculties encountered in the conventional manufacture of brake lining dusts. Comminution in the absence of oxygen precludes accidental combustion and attendant hazards. Further, grinding at room temperature is not practicable with rubbery materials, The practice of this invention eliminates the necessity for this step.

Referring to the drawing in order to more fully illustrate the invention, numeral I represents the reaction unit into which the oil is charged. Heat is supplied to the unit by gas burners 3 or other suitable heating means. Vigorous and continuous agitation is effected by means of rotary agitator 2. The reaction unit communicates with a condenser 4 and a rezeiver 5. To the receiver is connected a pump 6 which serves to produce and maintain the vacuum on the system,

The following examples are illustrative oi. the practice of this invention.

Example 1.2000 grams of linseed oil were heated under an absolute pressure of 2 inches of mercury or better to a maximum temperature of about 620 F. with continuous agitation until 350 grams were removed as distillate. 1600 grams of a comminuted, infusible, springy residuewere obtained.

Example 2.-2000 grams of sunflower oil were heated under an absolute pressure of 2 inches of mercury or better to a maximum temperature of about 620 F. with continuous agitation until 325 grams were removed as distillate. 1600 grams of residue were obtained.

The residue in this case was less springy and more highly comminuted than the linseed oil residue of Example 1.

Example 3.--l000 grams of sardine oil were heated similarly as above to a maximum temperature of about 655 F. until 275 grams were re moved as distillate. Solid residue was again obtained. I

Example 4.1000 grams of corn oil were heated similarly as above to a maximum temperature pressure conditions for a given run of material.

Pressures ranging downwardly'from 5, inches of mercury are operab1e.

I claim:

1. Method of obtaining a comminuted, infusible residue from a drying oil having an iodine number in excess of 120 (Wijs) and substantially free of conjugated double bonds which comprises distilling such an oil at a temperature between 610-700 F. under reduced pressure ranging downwardly from inches of mercury pressure and with continuous agitation until the quantity by weight of distillate removed therefrom measures between about to about 30% ofthe original mass by weight and said comminuted infusible residue measuring from 70-90%. by weight of the original oil is obtained.

2. Method of obtaining a comminuted, iniusible residue from linseed oil which comprises distilling said oil at a temperature between 610-700 F. under reduced pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation the quantity by weight of distillate removed therefrom being between about 10% to 30% of the original mass by weight and said comminuted infuslble residue measuring from 70-90% by weight of the original oil is obtained.

3. Method of obtaining a comminuted, infusible product from sunflower oil which comprises heating said oil at a temperature between 610-700 1". under reduced pressure ranging downward from 5 inches of mercury pressure and with continuous agitation until a residue of from 7090% by weight of the original oil is obtained.

4. Solid, polymerized product obtained from sunflower oil, said product characterized by being commi nuted and infusible and prepared by heating the oil at a temperature between 610-700 F. under reduced pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation until a residue of from 70-90% by weight of the original oil is obtained.

5. Method of obtaining a comminuted, infusible product from sardine oil which comprises heating said oil at a temperature between 610-700 F. under reduced pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation until a residue of from 70-90% by weight of the original oil is obtained.

6. Solid, polymerized product obtained from sardine oil, said product characterized by being ,comminuted and infusible and prepared by heating the oil at a temperature between 610-700 F. under reduced. pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation until a residue of from 70-90% by weight of the original oil is obtained.

7. A comminuted infusible residue obtained from a drying oil having an Iodine N0. in excess of 120 (Wijs) and substantially free of conjugated double bonds, said residue produced by distilling said oil at a temperature between 610 F. to about 700 F. under reduced pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation until the quantity of distillate removed therefrom is between about 10%-30% of the original mass by weight and said residue measuring between about %90% by weight of the original mass is obtained.

8. A comminuted infusible residue obtained from linseed oil by the method comprising heat in said oil at a temperaturebetween 610-700 F. under reduced pressure ranging downwardly from 5 inches of mercury pressure and with continuous agitation until the quantity by weight'of distillate removed therefrom is between about 10%-30% of the original mass of linseed oil by weight and said residue is obtaine WILLIAM F. SCHAUFELBERGER.

REFERENCES CITED The following references are of record in the file of this patent:

'UNITED STATES PATENTS Number Name Date 1,577,426 Schuricht Mar. 16, 1926 2,155,009 Fawcett Apr. 18, 1939 2,189,772 Auer Feb. 13, 1940 2,311,681 Morse Feb. 23, 1943 2,366,525 Harvey et a1. Jan..2, 1945 2,403,458 Ransom et al. July 9, 1946 OTHER REFERENCES Fisheries Research Board of Canada, Bulletin No. LIX, 1941, Chemistry and Technology, of Marine Animal Oils. Brocklesby. pages 124-131. 

